Pyrazole compound preparation method

A compound and pyrazole technology, applied in the field of preparation of pyrazole compounds, can solve the problems of low production efficiency and production cost, long reaction period, serious side reactions, etc., and achieve precise control of reaction conditions, shortened reaction time, and reduced The effect of by-product formation

Inactive Publication Date: 2017-06-06
LIANHE CHEM TECH TAIZHOU
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  • Abstract
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Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the problems of serious side reactions, long reaction cycle, low production efficiency and low production cost when using conventional synthetic methods to synthesize pyrazole compounds in the prior art, thus providing a method completely different from the prior art The preparation method of different pyrazole compounds, the preparation method of the present invention is carried out using a microchannel reactor, the reaction time is extremely short, the reaction conditions are controlled precisely, and the safety is high. It is suitable for rapid preparation of products, can be continuously produced, and has low cost. And the use of microchannel reactors to prepare pyrazole compounds has high reaction regioselectivity, good purity of target compounds, and is more suitable for large-scale industrial production

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0037]

[0038] 1. Raw material preparation: Weigh compound a (31.5g, 0.142mol) to configure its xylene solution (80.0mL), put it into a container, stir it to mix evenly and seal it, and put it in raw material tank 1; weigh compound b (40 % methylhydrazine aqueous solution, 17.2g, 0.149mol, 19.8mL), put in raw material tank 2;

[0039] 2, utilize the device of the present invention figure 2 , according to the following steps: (1) the xylene solution of compound a in raw material tank 1 enters Corning microchannel reactor 7 by metering pump 3, and the 40% methylhydrazine aqueous solution in raw material tank 2 enters Corning microchannel reactor by metering pump 4 Channel reactor 7; (2) setting each metering pump 3 and metering pump 4 to control the xylene solution and 40% methylhydrazine aqueous solution to be 20mL / min and 5.0mL / min respectively, and the heat exchanger temperature is set to 25°C, the reaction residence time is 240s; (3) Stop valves 5 and 6 are used to pre...

Embodiment 2

[0042]

[0043] 1. Preparation of raw materials: Weigh compound d (36.2g, 0.142mol) to prepare its toluene solution (180.0mL), put it into a container, stir to make it evenly mixed and sealed, and put it in raw material tank 1; weigh compound e (phenylhydrazine , 16.9g, 0.156mol), be mixed with its toluene suspension (60.0mL), be put in the raw material tank 2;

[0044] 2, utilize the device of the present invention figure 2 , according to the following steps: (1) the toluene solution of compound d in raw material tank 1 enters Corning microchannel reactor 7 by metering pump 3, and the toluene suspension of phenylhydrazine in raw material tank 2 enters Corning microchannel reactor by metering pump 4 Channel reactor 7; (2) setting each metering pump 3 and metering pump 4 to control the toluene solution of compound d and the toluene suspension of phenylhydrazine to be 30mL / min and 10.0mL / min respectively, and the heat exchanger temperature is set to 55°C, reaction residence...

Embodiment 3

[0047]

[0048] 1. Preparation of raw materials: Weigh compound g (41.6g, 0.200mol) to prepare its toluene solution (160.0mL), put it into a container, stir to mix it evenly and seal it, and put it in raw material tank 1; weigh compound b (40% Aqueous methylhydrazine solution, 24.2g, 0.210mol, 27.8mL), was placed in the raw material tank 2;

[0049] 2, utilize the device of the present invention figure 2 , according to the following steps: (1) the toluene solution of compound g in the raw material tank 1 enters the Corning microchannel reactor 7 through the metering pump 3, and the 40% methylhydrazine aqueous solution in the raw material tank 2 enters the Corning microchannel through the metering pump 4 Reactor 7; (2) set each metering pump 3 and metering pump 4 to control the toluene solution of compound g and 40% methylhydrazine aqueous solution to be 25mL / min and 4.3mL / min respectively, and set the heat exchanger temperature to be 40°C , reaction residence time 390s; (...

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Abstract

The invention discloses a preparation method of a pyrazole compound which is shown as a formula III. The preparation method disclosed by the invention comprises the following step of introducing a compound which is shown as a formula I and a compound which is shown as a formula II into a micro-channel reactor through different pipelines to react to obtain the pyrazole compound, wherein reaction temperature is 10 to 60 DEG C, R1 is C1-C4 alkyl, R2 and R3 are halogen independently, and R4 is methyl or phenyl. The preparation method disclosed by the invention is performed through the micro-channel reactor, has extremely-short reaction time, accurate reaction condition control and high safety, is suitable for quickly preparing products, achieves continuous production and has low cost; furthermore, the micro-channel reactor is utilized to prepare the pyrazole compound, so that reaction region selectivity is high, target compound purity is good, and the preparation method is more suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of pyrazole compounds. Background technique [0002] As an intermediate for the synthesis of other pharmaceutical compounds, pyrazole compounds are widely used in the fields of fine chemicals, medicine, and organic synthesis. [0003] The knorr dehydration condensation of hydrazine and 1,3-dicarbonyl compounds is a convenient general method for the synthesis of pyrazole compounds. This method is simple and efficient, and is widely used in the industrial production of pyrazole compounds. However, the regioselectivity problem in the knorr reaction itself makes its side reactions unavoidable, and there are many isomers, which seriously affect the products in its industrial production. Improved yield and purity. In addition, in industrial production, due to the large amount of heat released by the reaction system during the reaction process, local une...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/14
CPCC07D231/14
Inventor 潘强彪邹本立聂良邓高文罗艳妮
Owner LIANHE CHEM TECH TAIZHOU
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